CN103981573B - The method improving perovskite structure ferroelectric material Curie temperature - Google Patents
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Abstract
A kind of method improving perovskite structure ferroelectric material Curie temperature, it is characterised in that comprise the steps: that 1. materials synthesis is carried out in atmosphere, adds Mn in synthesis step2+Positive oxides, divalent as additive or after high-temperature process, become Mn2+, obtaining formula after dispensing is AB1‑xMnxO3Perovskite structure ferroelectric material；2. by the perovskite structure ferroelectric material aged at room temperature in atmosphere of above-mentioned acquisition or apply along monocrystalline<001>direction polarization.Compared with prior art, it is an advantage of the current invention that: use Mn2+Replacing B position batching mode, in conjunction with aging or<001>direction polarization so that the ferroelectric material Curie temperature of perovskite structure is significantly improved, the most overall processing cost is relatively low, and intractability is the least, beneficially popularization and application.
Description
Technical field
The present invention relates to a kind of perovskite structure ferroelectric material processing method.
Background technology
Ferroelectric material is that one has spontaneous polarization, and spontaneous polarization is under External Electrical Field, it is possible to occur again
The material of orientation.It is a very important electronic material of class, it is possible to be widely used in piezoelectric transducer, ferroelectricity
Memorizer, Infrared Detectors, the field such as piezoelectric transducer.Ferroelectric material can be block ceramic polycrystalline material,
Monocrystal material, the form such as thin film exists.Ferroelectric material has an important feature to be exactly that it has Curie temperature,
Below Curie temperature, ferroelectric material is ferroelectric phase, has spontaneous polarization.Exceed Curie temperature, ferroelectric material
Become Paraelectric cubic phase from tetragonal phase converting, lose the electrical property such as ferroelectricity, corresponding piezoelectricity, pyroelectric
Can all disappear.Therefore the height of Curie temperature is an important parameter index of ferroelectric material.
The material of perovskite structure is most important a kind of material in the middle of ferroelectric material, and his chemical general formula can be write
Become ABO3, A position can be Ca, and Ba, Pb, Bi, K, Na etc., in occupation of the vertex position of cubic cell；B
Position can be Ti, and Nb, Mg, Zn, In, Zr etc., in occupation of the position, body-centered of cubic cell；And O in occupation of
The center of area position of cubic cell, crystal structure is as shown in Figure 1.Utilize different element combinations can be formed not
Same ferroelectric material, such as: Pb (ZrxTi1-x)O3, BaTiO3,BaxCa1-xTiO3,
(1-x)(K1/2Na1/2)NbO3-xLiNbO3, (1-x) (Bi1/2Na1/2)TiO3-xBaTiO3,
(1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3, (1-x) Pb (Zn1/3Nb2/3)O3-xPbTiO3Deng.
The Curie temperature of the ferroelectric material of tradition preparation depends on the chemical composition of material, namely usual institute
The chemical method said.But improving Curie temperature when, along with the ferroelectric electrical property of perovskite structure
The decline of energy.Such as at (1-x) Pb (Zn1/3Nb2/3)O3-xPbTiO3In solid solution ferroelectric, along with PbTiO3Content increase,
Its Curie temperature increases, and when material is converted into four directions ferroelectric phase, its piezoelectric property is along with the biggest reduction.With
Other ferroelectric of sample also has similar character, electric property and Curie temperature seemingly contradiction.But physical method
The Curie temperature of material can be improved further, namely after the chemical composition of material is fixed up, when in use
The Curie temperature of material can be improved by adding extra electric field and stress etc. to ferroelectric material, but this method often makes
Ferroelectric material is greatly increased difficulty and the use cost of use application when.It is therefore desirable to invention is a kind of simple
Physical method improves the Curie temperature of ferroelectric material.
Summary of the invention
The technical problem to be solved is to provide one can improve perovskite structure for the above-mentioned state of the art
The method of ferroelectric material Curie temperature.
The present invention solves the technical scheme that above-mentioned technical problem used: a kind of improve perovskite structure ferroelectric material Curie
The method of temperature, it is characterised in that comprise the steps:
1. materials synthesis is carried out in atmosphere, adds Mn in synthesis step2+Positive oxides, divalent as additive or
Person becomes Mn after high-temperature process2+, obtaining formula after dispensing is AB1-xMnxO3Perovskite structure ferroelectric material,
This perovskite structure ferroelectric material has Lacking oxygen to produce, and the A in this formula occupies the vertex position of cubic cell, and A is
At least one in Ca, Ba, Pb, Bi, K, Na；B in this formula occupies the position, body-centered of cubic cell,
B is Ti, at least one in Nb, Mg, Zn, In, Zr；O in this formula occupies the center of area of cubic cell
Position；Mn in this formula2+The dispensing of Substitute For Partial B position；X in this formula meets: 0.03 >=x >=0.01,
Big doping solubility with occur without non-perovskite structure in the material material as criterion；
2. by the perovskite structure ferroelectric material aged at room temperature in atmosphere of above-mentioned acquisition or apply along monocrystalline<001>
Direction polarization.
As preferably, step 1. described in formula AB1-xMnxO3Corresponding ferroelectric material ABO3For Tetragonal ferroelectricity material
During material, step 2. in use aged at room temperature in atmosphere, described Tetragonal ferroelectric material at room temperature have grand farmland four directions
Phase, the spontaneous polarization direction in farmland is<001>direction.Further, described Tetragonal ferroelectric material is polycrystalline ceramics material
Material or multidomain ferro-electricity single crystal.
As preferably, described Tetragonal ferroelectric material is BaTiO3Or Ba0.85Ca0.15Zr0.1Ti0.9O3。
For Ba0.85Ca0.15Zr0.1Ti0.9O3Can use preferred steps:
Use pure BaCO3, CaCO3, ZrO2, TiO2, MnCO3, weigh 7.526g, 0.673g respectively,
0.547g, 3.198g, 0.069g put into mixing and ball milling in ball grinder, ball milling condition: the volume of raw material, Achates
Sphere volume, the volume ratio of ball-milling medium dehydrated alcohol are 1:1:1.5, by its ball milling 10 hours, after ball milling
Raw material is put into baking oven and is dried 5 hours at 80 DEG C；Raw material after drying utilize tablet machine at 20Mpa lower sheeting Cheng Zhi
The raw material idiosome of footpath 40mm, the raw embryo after having pressed slice puts into pre-burning in batch-type furnace, and pre-burning condition is 1200 DEG C of guarantors
Temperature 4 hours, pulverizes the bulk sample of synthesis, clays into power and sieve, and by its ball milling 10 hours, is placed again into
Within at 80 DEG C of baking oven 5 hours, dry；Finally, the powder after drying adds 1ml PVA (polyvinyl alcohol) by 10g powder and glues
The ratio of mixture is ground, and wears into uniform powder, sieves 3 times by 80 mesh sieve, and the weighing quality of milled powder is
0.500 gram, depress to the small pieces of a diameter of 13mm at 2MPa, at Al2O3The ZrO of 98% is spread on pad2Powder,
And with ZrO2The small pieces pressed are covered by powder, put it in batch-type furnace and sinter, and sintering condition is 1450 DEG C of insulations 4
Hour；After high-temperature process ceramic room temperature be Tetragonal Ba0.85Ca0.15(Zr0.1Ti0.9)0.99Mn0.01O3.By pottery
Sheet is put in atmosphere, aged at room temperature, ageing time 1 day～15 days.
Synthesis phase at material uses Mn2+Positive oxides, divalent as additive, the when of dispensing use add
Agent replaces the mode dispensing of B position, i.e. AB1-xMnxO3Dispensing, wherein maximum for x doping solubility is not to go out
The material of existing non-perovskite structure is criterion.In the preparation process of material, the chemical reaction related to is the most in atmosphere
Carry out.According to electricity price equilibrium principle, the B of+4 valencys4+The Mn of quilt+divalent2+Replace, in order to keep the electric neutrality of material,
Prepared by ferroelectric material out Lacking oxygen will be had to produce, namely the chemical formula of the material of preparation is write as: AB1-xMnxO3-x。
The Lacking oxygen of the ferroelectric material just prepared 6 centroid structures in cubic cell are random distributions, namely lack
Fall into dipoleSix<001>direction random orientations towards structure cell.Disfigurement model is if in ferroelectricity
Towards a specific direction arrangement in material, namelyDisfigurement model is ordered into arrangement, forms defective even
The most sub-D', disfigurement model D' are equivalent to be applied with an extra electric field to material, and the Curie temperature causing material is increased by this
Add.Ferroelectric is from low-temperature heat to high temperature Curie temperature, and ferroelectric is from ferroelectricity tetragonal phase converting one-tenth cube paraelectric phase, and ferrum
The spontaneous polarization direction of electricity Tetragonal is<001>direction, and ferroelectric Curie temperature will be made to increase, ferroelectric Disfigurement model must be orderly along<001>direction arrangement.According to the different characteristics of host material, the thing of post processing
Reason method is the most different.
(2) according to the elaboration of (1), for the normal ferroelectric material that room temperature is Tetragonal, such as BaTiO3, and solid solution
Body Ba0.85Ca0.15Zr0.1Ti0.9O3Deng, it has grand farmland Tetragonal in room temperature, and the spontaneous polarization direction in farmland is<001>
Direction, for the ferroelectricity multidomain material just prepared, due to disfigurement modelAt random along 6 in farmland
<001>direction arrangement, so for forming the dipole polarization intensity of macroscopic view in farmland.But it is placed on aged at room temperature, due to
Spontaneous polarization forms built in field, Lacking oxygen under the effect of built in fieldMigrate in ferroelectric domain so that defective even
Extremely sonOrientation the same with spontaneous polarization direction, it is established that spontaneous polarization strength direction and disfigurement model
Direction.The disfigurement model alignedAlso form built in field, and built-in electric field will stablize ferroelectric phase,
Thus obtain higher Curie temperature.Due to built in field can be spontaneous carry out in ferroelectric domain, so described material
Can be polycrystalline ceramic or multidomain ferro-electricity single crystal.
As preferably, step 1. described in formula AB1-xMnxO3Corresponding ferroelectric material ABO3For Pb-Based Relaxor Ferroelectric Materials
Time, step 2. middle employing applies along monocrystalline<001>direction polarization.Further, described Pb-Based Relaxor Ferroelectric Materials is
(1-x1)Pb(Mg1/3Nb2/3)O3-x1PbTiO3, x1≤0.35, (1-x2) Pb (Zn1/3Nb2/3)O3-x2PbTiO3, x2≤0.09.
Ferroelectricity para-electric changes and occurs a bigger temperature range, and this kind of material is relaxation phase in room temperature, and they do not have
There is grand domain structure, so the built in field of spontaneous polarization can not make Lacking oxygenMigrate in ferroelectric domain, thus by old
Change can not set up defect electric field.So that disfigurement modelArrangement can be along ferroelectricity Tetragonal
<001>direction arrangement, so electric field should be applied along<001>direction so thatMigrate in ferroelectric domain, thus build
Erect orderly disfigurement model.Owing to pottery is polycrystalline material, it is impossible to apply along specific<001>orientation
Built in field, so for relaxation ferroelectric, can only realize utilizing additional electric field polarization on monocrystal so that polarization
After positive bivalence Mn2+The Curie temperature of the relaxor ferroelectric monocrystal replacing B position increases.
Further, step 2. middle spontaneous polarization direction<001>direction that direction is ferroelectricity Tetragonal applying electric field, and
Polarized electric field is 0.2～2kV/mm.
For 0.95Pb (Zn1/3Nb2/3)O3-0.05PbTiO3Can use preferred steps:
By pure PbO, MgO, Nb2O5, TiO2According to 0.95Pb (Zn1/3Nb2/3)O3-0.05PbTiO3In raw material
Stoichiometric proportion dispensing, the when of dispensing, adds MnCO3As additive, Mn is made to replace
0.95Pb(Zn1/3Nb2/3)O3-0.05PbTiO3Mg in crystal, Nb, Ti, substitution amount is 0.3% molar content；By institute
The raw material joined is sufficiently mixed, and being then sealing in is directly the platinum crucible of 55 millimeters, utilizes
0.95Pb(Zn1/3Nb2/3)O3-0.05PbTiO3For seed crystal, grow along<111>direction, raw material 1300～1400 DEG C of materials,
Then utilizing the velocity pull-down of degrowth stove instrument 1-2mm per hour, the crystal grown out is just that 0.3% mole of manganese is mixed
Miscellaneous B position substituted 0.95Pb (Zn1/3Nb2/3)0.997Mn0.003O2.997-0.05PbTi0.997Mn0.003O3, by grow
0.95Pb(Zn1/3Nb2/3)0.997Mn0.003O2.997-0.05PbTi0.997Mn0.003O3Monocrystalline utilizes position finder to orient, and makes<001>
Direction, at room temperature, gives the electric field 30 minutes that<001>single-chip of being orientated applies a 1kV/mm.
Compared with prior art, it is an advantage of the current invention that: use Mn2+Replace B position batching mode, in conjunction with aging or
<001>direction polarization so that the ferroelectric material Curie temperature of perovskite structure is significantly improved, the most overall place
Reason cost is relatively low, and intractability is the least, beneficially popularization and application.
Accompanying drawing explanation
Fig. 1 is the crystal structure schematic diagram of perovskite in prior art.
Fig. 2 is the crystal structure schematic diagram of the substituted rear perovskite in B position in embodiment 1.
Fig. 3 is the crystal structure schematic diagram of the perovskite of disfigurement model orderly in embodiment 1.
Fig. 4 is the relation signal in the ferroelectric material just prepared in embodiment 1 between domain structure and disfigurement model
Figure.
Fig. 5 is in embodiment 1 in the ferroelectric material of the disfigurement model of ordered arrangement between domain structure and disfigurement model
Relation schematic diagram.
(Ba in Fig. 6 embodiment 10.85Ca0.15(Zr0.1Ti0.9)0.99Mn0.01O3Aging 15 days of potsherd and unaged sample
Dielectric temperature spectrum comparison diagram.
Detailed description of the invention
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment 1, uses the BaCO of purity 99.95%3, the CaCO of 99.99%3, the ZrO of 99.99%2,
The TiO of 99.8%2, analytically pure MnCO3Raw material, weigh 7.526g, 0.673g, 0.547g, 3.198g respectively,
0.069g puts into mixing and ball milling in ball grinder, ball milling condition: the volume of raw material, agate ball volume, ball-milling medium
The volume ratio of dehydrated alcohol is approximately equal to 1:1:1.5, and by its ball milling 10 hours, baking put into by the raw material after ball milling
Case dries 5 hours at 80 DEG C.Then, tablet machine is utilized to become diameter 40mm at 20Mpa lower sheeting raw material after drying
Raw material idiosome, the raw embryo after having pressed slice puts into pre-burning in KBF1700 batch-type furnace, and pre-burning condition is 1200 DEG C
It is incubated 4 hours, the bulk sample of synthesis is pulverized, clays into power and sieve, by its ball milling 10 hours, again put
Enter at 80 DEG C of baking oven 5 hours and dry.Finally, the powder after drying adds 1ml PVA (polyvinyl alcohol) by 10g powder
The ratio of binding agent is ground, and wears into uniform powder, sieves 3 times by 80 mesh sieve, the weighing quality of milled powder
It is 0.500 gram, depresses to the small pieces of a diameter of 13mm at 2MPa, at Al2O3The ZrO of 98% is spread on pad2
Powder, and with ZrO2The small pieces pressed are covered by powder, put it in batch-type furnace and sinter, and sintering condition is 1450 DEG C
It is incubated 4 hours.After high-temperature process ceramic room temperature be Tetragonal Ba0.85Ca0.15(Zr0.1Ti0.9)0.99Mn0.01O3。
Potsherd is put in atmosphere, aged at room temperature, after the aging different time, utilize Jie of electric impedance analyzer test potsherd
Electro-temperature is composed, and the temperature corresponding to dielectric constant maximum is the Curie temperature of ferroelectric ceramic material.Can from Fig. 6
The Curie temperature T of material after going out aging 15 dayscRatio is aged for one day big 3 DEG C of the Curie temperature of material, description defect dipole
After aged at room temperature, disfigurement model aligns in ferroelectric domain, by this aging effect, ferroelectricity
Ba0.85Ca0.15(Zr0.1Ti0.9)0.99Mn0.01O3The Curie temperature of pottery is strengthened.
In the preparation process of material, the chemical reaction related to is carried out the most in atmosphere.According to electricity price equilibrium principle,
The B of+4 valencys4+The Mn of quilt+divalent2+Replacing, in order to keep the electric neutrality of material, prepared ferroelectric material out will have
Lacking oxygen produces, namely the chemical formula of the material of preparation is write as: Ba0.85Ca0.15(Zr0.1Ti0.9)0.99Mn0.01O2.99.Just
The Lacking oxygen of the ferroelectric material prepared 6 centroid structures in cubic cell are random distributions, namely defective even
Extremely sonTowards six<001>direction random orientations of structure cell, its crystal structure is as shown in Figure 2. Disfigurement model if towards the arrangement of specific direction in ferroelectric material, as it is shown on figure 3, namelyLack
Sunken dipole, is ordered into arrangement, forms disfigurement model D', disfigurement model D' and is equivalent to be applied with outside one to material
Added electric field, the Curie temperature causing material is increased by this.Ferroelectric from low-temperature heat to high temperature Curie temperature, ferroelectric from
Ferroelectricity tetragonal phase converting becomes cube paraelectric phase, and the spontaneous polarization direction of ferroelectricity Tetragonal is<001>direction, ferrum to be made
The Curie temperature of electricity body increases, ferroelectricDisfigurement model must be orderly along<001>direction arrangement.
According to the different characteristics of host material, the physical method of post processing is the most different.
Ba0.85Ca0.15Zr0.1Ti0.9O3Having grand farmland Tetragonal in room temperature, the spontaneous polarization direction in farmland is<001>direction,
For the ferroelectricity multidomain material just prepared, due to disfigurement modelAt random along 6<001>in farmland
Direction arranges, so for forming the dipole polarization intensity of macroscopic view, its spontaneous polarization direction and disfigurement model in farmland
Direction is as shown in Figure 4.But it is placed on aged at room temperature, owing to spontaneous polarization forms built in field, in the effect of built in field
Lower Lacking oxygenMigrate in ferroelectric domain so that disfigurement modelOrientation and spontaneous polarization direction one
Sample, it is established that spontaneous polarization strength direction and disfigurement model direction as shown in Figure 5.The disfigurement model alignedAlso form built in field, and built-in electric field will stablize ferroelectric phase, thus obtain higher Curie temperature.By
In built in field can be spontaneous carry out in ferroelectric domain, so material can be polycrystalline ceramic or multidomain ferroelectricity list
Brilliant.
Embodiment 2, by high-purity PbO, MgO, Nb2O5, TiO2According to 0.95Pb (Zn1/3Nb2/3)O3-0.05PbTiO3
In raw material stoichiometric proportion dispensing, the when of dispensing, add MnCO3As additive, Mn is made to replace
0.95Pb(Zn1/3Nb2/3)O3-0.05PbTiO3Mg in crystal, Nb, Ti, substitution amount is 0.3% molar content.By institute
The raw material joined is sufficiently mixed, and being then sealing in is directly the platinum crucible of 55 millimeters, utilizes
0.95Pb(Zn1/3Nb2/3)O3-0.05PbTiO3For seed crystal, grow along<111>direction, raw material 1300～1400 DEG C of materials,
Then utilizing the velocity pull-down of degrowth stove instrument 1-2mm per hour, the crystal grown out is just that 0.3% mole of manganese is mixed
Miscellaneous B position substituted 0.95Pb (Zn1/3Nb2/3)O3-0.05PbTiO3Monocrystalline, namely can be write as chemical formula
0.95Pb(Zn1/3Nb2/3)0.997Mn0.003O2.997-0.05PbTi0.997Mn0.003O2.997.By grow
0.95Pb(Zn1/3Nb2/3)0.997Mn0.003O2.997-0.05PbTi0.997Mn0.003O2.997Monocrystalline utilizes position finder to orient, and makes
<001>direction, then utilizes inner circle cutting machine to be cut by monocrystalline, and is ground by single-chip, by upper silver electrode.Utilize resistance
The dielectric temperature spectrum of the crystal wafer that analysis resistant instrument test<001>is orientated, the temperature corresponding to dielectric constant maximum is ferrum
The Curie temperature of the material that electricity<001>is orientated.<001>Curie temperature of direction single-chip dielectric temperature spectrum display material is 175
DEG C, monocrystalline becomes cube paraelectric phase from ferroelectricity tetragonal phase converting.Due to
0.95Pb(Zn1/3Nb2/3)0.997Mn0.003O2.997-0.05PbTi0.997Mn0.003O2.997For relaxation ferroelectric, the list grown out
Brilliant farmland is nanometer domain structure.So that ferroelectric
0.95Pb(Zn1/3Nb2/3)0.997Mn0.003O2.997-0.05PbTi0.997Mn0.003O2.997In disfigurement modelOrientation
Spontaneous polarization direction<001>along Tetragonal ferroelectric domain arranges, and in room temperature, the single-chip being orientated to<001>applies one
The electric field of 1kV/mm 30 minutes, then the dielectric temperature spectrum of re-test material, the Curie temperature of dielectric temperature spectrum material increases
To 190 DEG C, compare unpolarized process the Curie temperature of crystal wafer add 20 DEG C.This demonstrate that and adulterated by Mn,
Then along<001>direction polarization, the Curie temperature of relaxor ferroelectric monocrystal can be increased.
Ferroelectricity para-electric changes and occurs a bigger temperature range, and this kind of material is relaxation phase in room temperature, and they do not have
There is grand domain structure, so the built in field of spontaneous polarization can not make Lacking oxygenMigrate in ferroelectric domain, thus by old
Change can not set up defect electric field.So that disfigurement modelArrangement can be along ferroelectricity Tetragonal
<001>direction arrangement, so electric field should be applied along<001>direction so thatMigrate in ferroelectric domain, thus build
Erect orderly disfigurement model.Owing to pottery is polycrystalline material, it is impossible to apply along specific<001>orientation
Built in field, so for relaxation ferroelectric, can only realize utilizing additional electric field polarization on monocrystal so that polarization
After positive bivalence Mn2+The Curie temperature of the relaxor ferroelectric monocrystal replacing B position increases.
Claims (1)
1. the method improving perovskite structure ferroelectric material Curie temperature, it is characterised in that comprise the steps:
Materials synthesis is carried out in atmosphere, uses pure BaCO3, CaCO3, ZrO2, TiO2, MnCO3Weigh 7.526g respectively, 0.673g, 0.547g, 3.198g, 0.069g put into mixing and ball milling in ball grinder, ball milling condition: the volume of raw material, agate ball volume, the volume ratio of ball-milling medium dehydrated alcohol are 1:1:1.5, by its ball milling 10 hours, the raw material after ball milling was put into baking oven and is dried 5 hours at 80 DEG C；After drying, raw material utilizes tablet machine to become the raw material idiosome of diameter 40mm at 20Mpa lower sheeting, a raw embryo after having pressed slice puts into pre-burning in batch-type furnace, pre-burning condition is 1200 DEG C and is incubated 4 hours, the bulk sample of synthesis is pulverized, clay into power and sieve, by its ball milling 10 hours, it is placed again at 80 DEG C of baking oven 5 hours drying；Finally, the ratio that the powder after drying adds 1ml poly (vinyl alcohol) binder in 10g powder is ground, and wears into uniform powder, sieves 3 times by 80 mesh sieve, and the weighing quality of milled powder is 0.500 gram, depresses to the small pieces of a diameter of 13mm at 2MPa, at Al2O3The ZrO of 98% is spread on pad2Powder, and with ZrO2The small pieces pressed are covered by powder, put it in batch-type furnace and sinter, and sintering condition is 1450 DEG C and is incubated 4 hours；Ceramic room temperature after high-temperature process is Tetragonal Ba0.85Ca0.15(Zr0.1Ti0.9)0.99Mn0.01O3, potsherd is put in atmosphere, aged at room temperature, ageing time 1 day ~ 15 days.
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